CN103665067A - Separation and purification method for Thonningianin A monomer - Google Patents
Separation and purification method for Thonningianin A monomer Download PDFInfo
- Publication number
- CN103665067A CN103665067A CN201310715198.7A CN201310715198A CN103665067A CN 103665067 A CN103665067 A CN 103665067A CN 201310715198 A CN201310715198 A CN 201310715198A CN 103665067 A CN103665067 A CN 103665067A
- Authority
- CN
- China
- Prior art keywords
- thonningianin
- monomer
- separation
- product
- ethanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a separation and purification method for a Thonningianin A monomer and belongs to the technical field of separation and purification of active components of traditional Chinese medicines. The separation and purification method comprises the specific steps of (1) extraction: cutting penthorum chinense pursh into small pieces, performing backflow extraction on the small pieces through ethanol, and then filtering the small pieces; (2) concentration: concentrating filtrate to 20 percent; (3) enrichment and elution of macroporous adsorption resin; (4) enrichment and elution of polyamide resin; (5) high-efficiency preparation and liquid chromatographic separation, wherein the flowing phase is an acetonitrile-3% phosphoric acid aqueous solution, and the detection wavelength is 254nm; (6) product recycling: filtering a Thonningianin A monomer solution to separate out crystals, and drying the crystals to obtain the Thonningianin A monomer product. The separation and purification method is easy and convenient to operate, short in production period, high in separation efficiency, stable and reliable in technology and high in reproducibility; the cost is easy to control, and the product is high in purity; the Thonningianin A monomer can be used as a standard substance for measuring the content.
Description
Technical field
The present invention relates to the separating and purifying method of medicinal plant compound monomer, specifically, relate to a kind of from Penthorum chinense the method for separation and purification Thonningianin A monomer, belong to Chinese medicine separating and purifying technology field.
Background technology
Penthorum chinense (Penthorum chinense Pursh) is the dry aerial parts of Saxifragaceae (Saxifragaceae) penthorum (Penthorum) plant Herba Lysimachiae Clethroids (Penthorum chinense Pursh).Summer, autumn gather, and remove impurity, dry or using fresh herb.Penthorum chinense is Miao ethnic group's conventional medicament, among the people with its all herbal medicine.Herb is warm in nature, taste is sweet, nontoxic, tool heat-clearing, diuresis elimination of urine, detoxify, invigorate blood circulation, flat liver, invigorating the spleen, the effects such as jaundice of dispelling.Cure mainly jaundice, oedema, through closing, under metrorrhagia, band, wound, and various hepatitis, cholecystitis, fatty liver etc.
Thonningianin A is the characteristic constituents of Penthorum chinense, is also the highest active flavonoid glycoside composition in this plant; Thonningianin A molecular formula is C
42h
34o
21, molecular weight is 874.16, its structural formula is as follows:
Because Thonningianin A is the characteristic constituents of Penthorum chinense, if therefore can using the quality evaluation index of Thonningianin A as this medicinal material and related preparations thereof, can reflect more truly that its quality has again specificity, also can play an important role to the quality control of Penthorum chinense medicinal material and preparation thereof simultaneously.
By lot of documents, retrieve discovery, at present only relevant for the report of total flavone extracting process in Penthorum chinense, as " the > > of < < South China Science & Engineering University 2012, the isolation identification of Penthorum chinense effective constituent and activity thereof and Study on extraction ".And have no relevant report for isolate high purity Thonningianin A monomer product from Penthorum chinense.
?
Summary of the invention
The object of the present invention is to provide a kind of separation purification method of Thonningianin A monomer.The method is easy and simple to handle, with short production cycle, separation efficiency is high, process stabilizing, cost is easy to control, can realize the high purity separation preparation of a large amount of Thonningianin A monomers, and the Thonningianin A monomer purity obtaining is high, can be used as content measuring standard material, and the quality of Penthorum chinense medicinal material and preparation thereof is control effectively.
In order to realize foregoing invention object, the technical solution used in the present invention is as follows:
A separation purification method for Thonningianin A monomer, comprises following processing step:
(1) extract
Penthorum chinense medicinal material is cut into the segment of 0.5cm, according to medicinal material weight: ethanolic soln=1Kg:6L, adds 70% ethanolic soln, refluxing extraction 3 times, each 2 hours, extracting liquid filtering, collection, merging filtrate;
According to the ratio of 1:6, both can effectively soak medicinal material, use ethanol consumption that again can be less, thereby the use cost of reduction solvent; And adopt 70% alcohol reflux, and both this flavones ingredient of Thonningianin A effectively can have been extracted, make again other impurity component solubility rates lower, while guaranteeing to prepare, impurity disturbs few.
(2) concentrated
By the filtrate recycling ethanol of step (1) collection, merging, be concentrated into the 15-25% of former filtrate volume, reduce the ethanol content in concentrated solution;
By concentrated, not only recyclable ethanol but also reduced the volume of pregnant solution in subsequent step.
(3) macroporous adsorbing resin for purification and wash-out
Filtrate after step (2) is concentrated is crossed macroporous adsorbent resin and is adsorbed, and by purified water, cleans resin to after colourless, then uses the ethanol elution product section of 60%-70%, colourless to effluent liquid, collects and merges elutriant, by elutriant concentrating under reduced pressure, reclaims ethanol;
By purified water, guarantee to remove large polar impurity and some carbohydrate contents, and 60-70% ethanol guarantee product by wash-out out in, the impurity that polarity is less but can not be eluted.
(4) polyamide resin enrichment and wash-out
Elutriant after step (3) is concentrated is crossed polyamide resin and is adsorbed, first with 10% ethanol clean resin extremely colourless after, then the ethanol elution product that is 90% by concentration, colourless to effluent liquid, collect and merge elutriant, by elutriant concentrating under reduced pressure, must be containing the concentrated solution of product after recovery ethanol;
Elutriant, by the absorption of polyamide resin, can effectively reach separated Thonningianin A and the effect of removing a part of impurity; And by 10% ethanol elution, falling pigment and the impurity of some large polarity, the impurity while reducing preparation disturbs; 90% ethanol is wash-out product fast, when concentrated, raw materials can be reduced to minimal volumes again.
(5) high performance preparative liquid chromatography is separated
Chromatographic condition is as follows:
Filler is C
18chromatographic column;
Mobile phase composition is: acetonitrile-0.3%(V/V) phosphate aqueous solution, and the two volume ratio is 45:55;
Detection wavelength is 254nm;
The elutriant of getting after step (4) concentrates adopts 0.45 μ m organic membrane filter with solvent filter, filtrate sample introduction, the preparation of carrying out Thonningianin A monomer is separated, UV-detector on-line monitoring, what specific aim was collected Thonningianin A monomer prepares cut solution, obtains Thonningianin A monomer solution;
Before carrying out high performance preparative liquid chromatography separation, can determine by the coupling of liquid-matter or the conventional method of other the art the peak shape of Thonningianin A monomer in high performance liquid chromatography.
Liquid-matter method for combined use of take is example, can be identical with above-mentioned preparation separation chromatography condition, and adopt chromatographic column that filler is identical, form identical moving phase, identical detection wavelength etc., column temperature is room temperature; The concentrated solution of getting step (4) gained filters, and then sample introduction, carries out the high performance liquid phase separation and purification of Thonningianin A monomer, according to mass spectrometric detection result, can determine Thonningianin A monomer corresponding peak shape in liquid chromatography.
High performance preparative liquid chromatography can be to product sharp separation with respect to other conventional separation method (such as silicagel column wash-out is separated), and the yield of product is improved a lot.
(6) product reclaims
The Thonningianin A monomer solution heating recovery acetonitrile that step (5) high performance preparative liquid chromatography separation is obtained, Thonningianin A monomer is separated out in a large number in the aqueous solution, after placing room temperature, with funnel, filter crystallize out, cross filter solid in 65 ℃ dry 12 hours, obtain Thonningianin A monomer product.
The purity of described Thonningianin A monomer product is rechecked and is adopted inverse analysis type liquid chromatography (RP-HPLC) method, and chromatographic condition is as follows:
With C
18(octadecylsilane chemically bonded silica) is weighting agent; Acetonitrile-0.3% phosphate aqueous solution (volume ratio 45:55) of take is moving phase; Flow velocity 1.0mL/min; Detecting wavelength is 254 nm.
Described in step (1), (3), (4), the concentration of ethanol is volume percent.
Due to high performance liquid chromatography the purity of sample solution, color and luster etc. are required all higher, raw material need be processed to impurity as much as possible early stage and pigment less, so just can reach good separating effect.
In high performance liquid chromatography sepn process, the selection of chromatographic condition is extremely important, and it plays conclusive effect to the peak sequence of each material in sample solution, peak shape, separating effect etc.; Chromatographic condition mainly comprises chromatographic column (comprising filler, column length and internal diameter etc.), moving phase (comprise form and flow velocity etc.), detects wavelength, detector etc., and the selection of each chromatographic condition and combination also most important.
The present invention is by a large amount of experimental studies and comparative analysis, determined each chromatographic condition as above, make the appearance time, peak shape, separating effect etc. of each material in sample solution reach optimizing, thereby it is fully effectively separated to guarantee that Thonningianin A monomer obtains.
Compared with prior art, advantage of the present invention and useful technique effect are:
1, the present invention adopts preparative high performance liquid chromatography system to carry out separation and purification to Thonningianin A monomer, by optimum pre-treating process (extract, concentrated, macroporous adsorbing resin for purification and wash-out, polyamide resin enrichment and wash-out) and chromatographic condition etc., reach good separating effect, UV-detector on-line monitoring process is directly perceived, specific aim is collected Thonningianin A monomer, with clearly defined objective, and be easy to control quality product.
2, the present invention is easy and simple to handle, with short production cycle, and product yield is high, purity is up to more than 98%, and process stabilizing is reliable, favorable reproducibility, and cost is easy to control.
3, the equal recyclable recycling of the organic reagent in each processing step of the present invention, solvent-oil ratio is few.
4, there is higher learning value.Owing to not yet there being at present the report of energy large-scale production Thonningianin A monomer method; products obtained therefrom of the present invention not only can effectively improve the present situation that Thonningianin A reference substance lacks, and also can provide high purity high quality raw material for industrialization development Thonningianin A preparation.
Accompanying drawing explanation
Fig. 1 is that the HPLC of the embodiment of the present invention 1 Thonningianin A product analyzes collection of illustrative plates.
Fig. 2 is the high performance preparative liquid chromatography figure of the embodiment of the present invention 1, is recorded as 4 sample needle continuous sample introduction color atlass in figure.
Fig. 3 is that the HPLC that the Thonningianin A monomer product of the embodiment of the present invention 1 is rechecked analyzes collection of illustrative plates.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
But this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment.
In following each embodiment, the purity of finished product Thonningianin A monomer is rechecked and is all adopted inverse analysis type liquid chromatography (RP-HPLC) method, and chromatographic condition is as follows:
With C
18(octadecylsilane chemically bonded silica) is weighting agent; Acetonitrile-0.3% phosphate aqueous solution (45:55) of take is moving phase; Flow velocity 1.0mL/min; Detecting wavelength is 254 nm.
embodiment 1
(1) extract
Get 1 kilogram of segment that is cut into 0.5cm of Penthorum chinense medicinal material, adding 6L concentration is 70% ethanolic soln, refluxing extraction 3 times, and each 2 hours, filter, collect, merging filtrate;
(2) concentrated
The filtrate recycling ethanol that step (1) is collected, merged, being concentrated into volume is 3.5L;
(3) macroporous adsorbing resin for purification and wash-out
It is that the macroporous adsorption resin chromatography post of 10cm adsorbs that filtrate after step (2) is concentrated is crossed diameter, first by purified water, clean resin to after colourless, the ethanol elution product that is 60% by concentration again, colourless to effluent liquid, collect and merge elutriant 5L altogether, by elutriant concentrating under reduced pressure, reclaim ethanol, obtain concentrated solution 1.5L;
(4) polyamide resin enrichment and wash-out
It is that the polyamide resin chromatography column of 10cm adsorbs that the concentrated solution of step (3) gained is crossed to diameter, after enrichment is complete, after first 10% ethanol cleaning resin is extremely colourless, use again 90% ethanol elution product, colourless to effluent liquid, collect and merge elutriant 2.5L altogether, by elutriant concentrating under reduced pressure, reclaim ethanol, obtaining concentrated solution is 250mL;
(5) high performance preparative liquid chromatography is separated
Chromatographic condition is as follows:
Filler is C
18chromatographic column, post specification is 50cm * 10cm;
Mobile phase composition is: acetonitrile-0.3%(V/V) phosphate aqueous solution, and volume ratio is 45:55;
Detection wavelength is 254nm, ambient operation;
The concentrated solution of getting step (4) gained adopts 0.45 μ m organic membrane filter with solvent filter, filtrate sample introduction, each pin sample size filtrate is 125mL, UV-detector on-line monitoring, what specific aim was collected Thonningianin A monomer prepares cut solution, obtains Thonningianin A monomer solution;
Before carrying out high performance preparative liquid chromatography separation, by liquid-matter method for combined use, determine the peak shape of Thonningianin A monomer in high performance liquid chromatography, the chromatographic condition adopting is the same, the concentrated solution of getting step (4) gained filters then sample introduction, carry out the high performance liquid phase separation and purification of Thonningianin A monomer, according to mass spectrometric detection result, determine Thonningianin A monomer corresponding peak shape in liquid chromatography;
(6) product reclaims
50 ℃ of heating recovery acetonitriles of Thonningianin A monomer solution that step (5) high performance preparative liquid chromatography separation is obtained, obtain separating out product water solution 800mL, after placing room temperature, with funnel, filter Thonningianin A crystal, cross filter solid in 65 ℃ dry 12 hours, obtain 0.26 gram of honningianin A monomer product.HPLC analyzes collection of illustrative plates as shown in Figure 1.
Approximately 4 days whole Production Flow Chart used times.
Calculating product yield is (0.26/1000) * 100%=0.026%.
By changing mobile phase composition, utilize inverse analysis type liquid chromatography (RP-HPLC) to recheck product purity, recording result is 99.20%.
embodiment 2
(1) extract
Get 10 kilograms of segments that are cut into 0.5cm of Penthorum chinense medicinal material, adding 60L concentration is 70% ethanolic soln, refluxing extraction 3 times, and each 2 hours, filter, collect, merging filtrate;
(2) concentrated
The filtrate recycling ethanol that step (1) is collected, merged, being concentrated into volume is 35L.
(3) macroporous adsorbing resin for purification and wash-out
It is that the macroporous adsorption resin chromatography post of 10cm adsorbs that filtrate after step (2) is concentrated is crossed diameter, first by purified water, clean resin to after colourless, the ethanol elution product that is 70% by concentration again, colourless to effluent liquid, collect and merge elutriant 5L altogether, by elutriant concentrating under reduced pressure, reclaim ethanol, obtain concentrated solution 14L;
(4) polyamide resin enrichment and wash-out
It is that the polyamide resin chromatography column of 15cm adsorbs that the concentrated solution of step (3) gained is crossed to diameter, after enrichment is complete, first with 10% ethanol, clean resin to after colourless, use again 90% ethanol elution product, colourless to effluent liquid, collect and merge elutriant 25L altogether, by elutriant concentrating under reduced pressure, reclaim ethanol, obtaining concentrated solution is 2.5L;
(5) high performance preparative liquid chromatography is separated
Chromatographic condition is as follows:
Filler is C
18chromatographic column, post specification is 50cm * 10cm;
Mobile phase composition is: acetonitrile-0.3%(V/V) phosphate aqueous solution, and volume ratio is 45:55;
Detection wavelength is 254nm, ambient operation;
The concentrated solution of getting step (4) gained adopts 0.45 μ m organic membrane filter with solvent filter, filtrate sample introduction, each pin sample size filtrate is 125mL, UV-detector on-line monitoring, what specific aim was collected Thonningianin A monomer prepares cut solution, obtains Thonningianin A monomer solution;
Before carrying out high performance preparative liquid chromatography separation, by liquid-matter method for combined use, determine the peak shape of Thonningianin A monomer in high performance liquid chromatography, the chromatographic condition adopting is the same, the concentrated solution of getting step (4) gained filters then sample introduction, carry out the high performance liquid phase separation and purification of Thonningianin A monomer, according to mass spectrometric detection result, determine Thonningianin A monomer corresponding peak shape in liquid chromatography;
(6) product reclaims
The Thonningianin A monomer solution heating recovery acetonitrile that step (5) high performance preparative liquid chromatography separation is obtained, obtain separating out product water solution 800mL, after placing room temperature, with funnel, filter Thonningianin A crystal, cross filter solid in 65 ℃ dry 12 hours, obtain 2.82 grams of honningianin A monomer products.
Approximately 5 days whole Production Flow Chart used times.
Calculating product yield is (2.82/100000) * 100%=0.0282%.
By changing mobile phase composition, utilize inverse analysis type liquid chromatography (RP-HPLC) to recheck product purity, recording result is 99.12%.
embodiment 3
(1) extract
Get 50 kilograms of segments that are cut into 0.5cm of Penthorum chinense medicinal material, adding 300L concentration is 70% ethanolic soln, refluxing extraction 3 times, and each 2 hours, filter, collect, merging filtrate;
(2) concentrated
The filtrate recycling ethanol that step (1) is collected, merged, being concentrated into volume is 180L.
(3) macroporous adsorbing resin for purification and wash-out
It is that the macroporous adsorption resin chromatography post of 25cm adsorbs that filtrate after step (2) is concentrated is crossed diameter, first by purified water, clean resin to after colourless, the ethanol elution that is 65% by concentration again, colourless to effluent liquid, collect and merge elutriant 220L altogether, by elutriant concentrating under reduced pressure, reclaim ethanol, obtain concentrated solution 14L;
(4) polyamide resin enrichment and wash-out
It is that the polyamide resin chromatography column of 25cm adsorbs that the concentrated solution of step (3) gained is crossed to diameter, after enrichment is complete, first with 10% ethanol, clean resin to after colourless, use again 90% ethanol elution product, colourless to effluent liquid, collect and merge elutriant 120L altogether, by elutriant concentrating under reduced pressure, reclaim ethanol, obtaining concentrated solution is 12L;
(5) high performance preparative liquid chromatography is separated
Chromatographic condition is as follows:
Filler is C
18chromatographic column, post specification is 50cm * 10cm;
Mobile phase composition is: acetonitrile-0.3%(v/v) phosphate aqueous solution, and volume ratio is 45:55;
Detection wavelength is 254nm, ambient operation;
The concentrated solution of getting step (4) gained adopts 0.45 μ m organic membrane filter with solvent filter, filtrate sample introduction, each pin sample size filtrate is 125mL, UV-detector on-line monitoring, what specific aim was collected Thonningianin A monomer prepares cut solution, obtains Thonningianin A monomer solution;
Before carrying out high performance preparative liquid chromatography separation, by liquid-matter method for combined use, determine the peak shape of Thonningianin A monomer in high performance liquid chromatography, the chromatographic condition adopting is the same, the concentrated solution of getting step (4) gained filters then sample introduction, carry out the high performance liquid phase separation and purification of Thonningianin A monomer, according to mass spectrometric detection result, determine Thonningianin A monomer corresponding peak shape in liquid chromatography;
(6) product reclaims
The Thonningianin A monomer solution heating recovery acetonitrile that step (5) high performance preparative liquid chromatography separation is obtained, obtain separating out product water solution 30L, after placing room temperature, with funnel, filter Thonningianin A crystal, cross filter solid in 65 ℃ dry 12 hours, obtain 15.3 grams of honningianin A monomer products.
Approximately 5 days whole Production Flow Chart used times.
Calculating product yield is (15.3/5000000) * 100%=0.0306%.
By changing mobile phase composition, utilize inverse analysis type liquid chromatography (RP-HPLC) to recheck product purity, recording result is 98.89%.
Claims (3)
1. a separation purification method for Thonningianin A monomer, is characterized in that: comprise following processing step:
(1) extract
Penthorum chinense medicinal material is cut into the segment of 0.5cm, according to medicinal material weight: 70% ethanolic soln=1Kg:6L, adding concentration is 70% ethanolic soln, refluxing extraction 3 times, and each 2 hours, extracting liquid filtering, collected, merging filtrate;
(2) concentrated
By the filtrate recycling ethanol of step (1) collection, merging, be concentrated into the 15-25% of former filtrate volume;
(3) macroporous adsorbing resin for purification and wash-out
Filtrate after step (2) is concentrated is crossed macroporous adsorbent resin and is adsorbed, and first by purified water, cleans resin to after colourless, then uses the ethanol elution product of 60%-70%, colourless to effluent liquid, collects and merges elutriant, by elutriant concentrating under reduced pressure, reclaims ethanol;
(4) polyamide resin enrichment and wash-out
Elutriant after step (3) is concentrated is crossed polyamide resin and is adsorbed, first with 10% ethanol clean resin extremely colourless after, then use 90% ethanol elution product, colourless to effluent liquid, collect and merge elutriant, by elutriant concentrating under reduced pressure, reclaim ethanol and must resolve product concentrated solution;
(5) high performance preparative liquid chromatography is separated
Chromatographic condition is as follows:
Filler is C
18chromatographic column;
Mobile phase composition is: acetonitrile-0.3% phosphate aqueous solution, and the two volume ratio is 45:55;
Detection wavelength is 254nm;
Get step (4) concentrated solution and adopt 0.45 μ m organic membrane filter with solvent filter, filtrate sample introduction, the preparation of carrying out Thonningianin A monomer is separated, UV-detector on-line monitoring, what specific aim was collected Thonningianin A monomer prepares cut solution, obtains Thonningianin A monomer solution;
(6) product reclaims
The Thonningianin A monomer solution heating recovery acetonitrile that step (5) high performance preparative liquid chromatography separation is obtained, Thonningianin A monomer is separated out in a large number in the aqueous solution, after placing room temperature, with funnel, filter crystallize out, cross filter solid in 65 ℃ dry 12 hours, obtain Thonningianin A monomer product;
Described in step (1), (3), (4), the concentration of ethanol is volume percent.
2. the separation purification method of a kind of Thonningianin A monomer according to claim 1, it is characterized in that: before carrying out high performance preparative liquid chromatography separation, by liquid-matter method for combined use, determine the peak shape of Thonningianin A monomer in high performance liquid chromatography, the concentrated solution of getting step (4) gained filters then sample introduction, carry out the high performance liquid phase separation and purification of Thonningianin A monomer, according to mass spectrometric detection result, determine Thonningianin A monomer corresponding peak shape in liquid chromatography, chromatographic condition is as follows:
Filler is C
18chromatographic column;
Mobile phase composition is: acetonitrile-0.3% phosphate aqueous solution, and the two volume ratio is 45:55;
Detection wavelength is 254nm.
3. the separation purification method of a kind of Thonningianin A monomer according to claim 1, it is characterized in that: the purity of the described Thonningianin A of step (6) monomer product is rechecked and adopted inverse analysis type liquid chromatography RP-HPLC method, and chromatographic condition is as follows:
With C
18for weighting agent; Acetonitrile-0.3% phosphate aqueous solution the V/V=45:55 of take is moving phase; Flow velocity 1.0mL/min; Detection wavelength is 254nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310715198.7A CN103665067B (en) | 2013-12-23 | 2013-12-23 | A kind of separation purification method of Thonningianin A monomer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310715198.7A CN103665067B (en) | 2013-12-23 | 2013-12-23 | A kind of separation purification method of Thonningianin A monomer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103665067A true CN103665067A (en) | 2014-03-26 |
| CN103665067B CN103665067B (en) | 2015-10-21 |
Family
ID=50303928
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310715198.7A Active CN103665067B (en) | 2013-12-23 | 2013-12-23 | A kind of separation purification method of Thonningianin A monomer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103665067B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546872A (en) * | 2014-12-09 | 2015-04-29 | 华南理工大学 | Application of ellagitannins flavone in preparation of antitumor drugs |
| CN105193833A (en) * | 2015-10-13 | 2015-12-30 | 四川古蔺肝苏药业有限公司 | Application of penthorum chinense pursh monomer in preparation of liver protection medicine |
| CN108567789A (en) * | 2018-06-29 | 2018-09-25 | 浙江中医药大学 | Thonningianin A are preparing the application in preventing or treating alcoholic myocardiopathy drug |
| CN109260239A (en) * | 2018-11-08 | 2019-01-25 | 西南医科大学 | Penthorum chinense pursh general flavone preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177440A (en) * | 2007-10-12 | 2008-05-14 | 成都普思生物科技有限公司 | Method for rapid purification of codonopsis pilosula lobetyolin monomer from codonopsis pilosula medicinal materials |
| CN103242398A (en) * | 2013-04-26 | 2013-08-14 | 四川古蔺肝苏药业有限公司 | Dihydroflavone compound as well as preparation method and application for same |
-
2013
- 2013-12-23 CN CN201310715198.7A patent/CN103665067B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177440A (en) * | 2007-10-12 | 2008-05-14 | 成都普思生物科技有限公司 | Method for rapid purification of codonopsis pilosula lobetyolin monomer from codonopsis pilosula medicinal materials |
| CN103242398A (en) * | 2013-04-26 | 2013-08-14 | 四川古蔺肝苏药业有限公司 | Dihydroflavone compound as well as preparation method and application for same |
Non-Patent Citations (3)
| Title |
|---|
| IKUKO I. OHTANI, NAOMI GOTOH. ET AL.: "Thonningianins A and B, New Antioxidants from the African Medicinal Herb Thonningia sanguinea.", 《JOURNAL OF NATURAL PRODUCTS》, vol. 63, no. 5, 5 April 2000 (2000-04-05), pages 676 - 679 * |
| QUN LU. ET AL.: "Isolation and Identification of Compounds from Penthorum chinense Pursh with Antioxidant and Antihepatocarcinoma Properties.", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》, vol. 60, no. 44, 17 October 2012 (2012-10-17), pages 11097 - 11103 * |
| 冯浩, 等.: "赶黄草化学成分的研究.", 《中国中药杂志》, vol. 26, no. 4, 25 April 2001 (2001-04-25), pages 260 - 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546872A (en) * | 2014-12-09 | 2015-04-29 | 华南理工大学 | Application of ellagitannins flavone in preparation of antitumor drugs |
| CN105193833A (en) * | 2015-10-13 | 2015-12-30 | 四川古蔺肝苏药业有限公司 | Application of penthorum chinense pursh monomer in preparation of liver protection medicine |
| CN105193833B (en) * | 2015-10-13 | 2018-11-30 | 四川古蔺肝苏药业有限公司 | Penthorum chinense pursh monomer is preparing the purposes in Liver protection drug |
| CN108567789A (en) * | 2018-06-29 | 2018-09-25 | 浙江中医药大学 | Thonningianin A are preparing the application in preventing or treating alcoholic myocardiopathy drug |
| CN108567789B (en) * | 2018-06-29 | 2020-02-21 | 浙江中医药大学 | Application of Thonningianin A in preparation of drugs for preventing or treating alcoholic myocardial disease |
| CN109260239A (en) * | 2018-11-08 | 2019-01-25 | 西南医科大学 | Penthorum chinense pursh general flavone preparation method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103665067B (en) | 2015-10-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102451235B (en) | Preparation method of olive leaf extract | |
| CN102276679B (en) | Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling | |
| CN101260131A (en) | Method for extracting iridoid active site and monomer from eucommia bark | |
| CN101948501B (en) | Preparation method of hydroxyl asiaticoside | |
| CN108864217B (en) | Purification method of pomegranate peel punicalagin | |
| CN106967137B (en) | Method for separating high-purity oleuropein by liquid chromatography through macroporous resin combined preparation | |
| CN103665067B (en) | A kind of separation purification method of Thonningianin A monomer | |
| CN103483402A (en) | Method for purifying and preparing stevioside and rebaudioside-A | |
| CN101921277B (en) | Method for simultaneously preparing vasicine and vasicinone from peganum harmala | |
| CN105294628A (en) | Method for preparing flavonoid component by separating wild chrysanthemum flower | |
| CN101863935B (en) | Preparation method of 1,4-di-[4-(glucosyloxy) benzyl]-2-isobutyl malate comparison product | |
| CN102093328B (en) | Method for enriching and purifying procyanidin in pine bark | |
| CN103408610A (en) | Method for extracting arbutin from pear leaves | |
| CN103664842A (en) | Continuous chromatographic separation method for andrographolide | |
| CN109096351A (en) | A kind of buckeye saponin extraction technique | |
| CN102040635B (en) | Method for efficiently separating and purifying forsythiaside B monomer and poliumoside monomer | |
| CN103073605A (en) | Method for separating and purifying linarin monomers | |
| CN105434539A (en) | Composition of lotus flavones | |
| CN103655642A (en) | Method for preparing ginkgo biloba extract | |
| CN103083392B (en) | A kind of method at tool isoamylene radical chromocor position in separation and concentration Radix Sophorae Tonkinensis | |
| CN103059037B (en) | A kind of method of Chelidonine in enriching and purifying greater celandine | |
| CN102250174A (en) | Method for extracting jasminin from winter jasmine leaves | |
| CN102250183B (en) | Method for preparing high-purity ginsenoside Re by using ginseng flower buds as raw materials | |
| CN102399252A (en) | Preparation method for cowherb seed flavonoid glycoside monomer | |
| CN103070899B (en) | A kind of isolation and purification method of total Flavonoids from Taraxacum mongolicum |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 610045 Sichuan city of Chengdu province Wuhou District Wuhou New Town Road No. 8 West two CMC Vuko Patentee after: CHENGDU PUSH BIO-TECHNOLOGY CO., LTD. Address before: 610045 Sichuan city of Chengdu province Wuhou District Vuko two West Road No. 8 Patentee before: Pusi Biological Science & Technology Co., Ltd., Chengdu |
|
| CP03 | Change of name, title or address |